CN102181219A - Water-based anticorrosive coating of nano montmorillonite and polypyrrole complex and preparation method thereof - Google Patents
Water-based anticorrosive coating of nano montmorillonite and polypyrrole complex and preparation method thereof Download PDFInfo
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- CN102181219A CN102181219A CN 201110092265 CN201110092265A CN102181219A CN 102181219 A CN102181219 A CN 102181219A CN 201110092265 CN201110092265 CN 201110092265 CN 201110092265 A CN201110092265 A CN 201110092265A CN 102181219 A CN102181219 A CN 102181219A
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- nano imvite
- polypyrrole
- parts
- corrosion paint
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- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229910052901 montmorillonite Inorganic materials 0.000 title claims abstract description 18
- 238000000576 coating method Methods 0.000 title abstract description 12
- 239000011248 coating agent Substances 0.000 title abstract description 10
- 238000010668 complexation reaction Methods 0.000 title 1
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- 239000011347 resin Substances 0.000 claims abstract description 16
- 239000011159 matrix material Substances 0.000 claims abstract description 12
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- Paints Or Removers (AREA)
Abstract
The invention discloses a water-based anticorrosive coating of nano montmorillonite and polypyrrole complex and a preparation method thereof, and relates to a coating. The coating comprises the following raw materials in part by weight: 1 to 50 parts of montmorillonite, 20 to 300 parts of solvent, 0.8 to 55 parts of protonic acid, 0.07 to 18.5 parts of organic active agent, 8.5 to 50.6 parts of ferric trichloride hexahydrate or ferric sulfate, 0.8 to 56 parts of pyrrole, 4.5 to 50 parts of surfactant, 10 to 55 parts of resin matrix, 0 to 10 parts of modified resin, 0.34 to 5.6 parts of neutralizing agent, 0.6 to 10 parts of pigment, 20 to 100 parts of deionized water, 0.05 to 1.2 parts of defoaming agent, 0.22 to 1.34 parts of anti-settling agent, 0.13 to 1.15 parts of dispersant, 0.02 to 1.08 parts of flatting agent and 0.05 to 1.04 parts of film-forming auxiliary agent. The method comprises the following steps of: preparing the nano montmorillonite and polypyrrole complex, namely pre-treating the montmorillonite and synthesizing the nano montmorillonite and polypyrrole complex; and preparing the coating.
Description
Technical field
The present invention relates to a kind of coating, the nano imvite of particularly a kind of low cost, high Corrosion Protection and polypyrrole mixture watery anti-corrosion paint and preparation method thereof.
Background technology
In industries such as chemical industry, oil, food, light industry, most equipment, pipeline are usually caused damage by various corrosive medium corrosion.For hardware and corrosive medium are isolated fully, prevent that it is corroded and denudes, improve solidity to corrosion, wear resistance, security and the work-ing life of equipment, people make tectum or lining with various anticorrosion materials usually.In various aseptic technics, anticorrosion with coat erosion technology is most widely used general, because its easy construction, wide adaptability, the constraint that is not subjected to device area, shape, recoat and reparation aspect expense are low, anticorrosion with coat also can be united use with other anticorrosive measure.In addition, in marine ship industry, prevent that sea marine organism pollution and marine corrosion from being a bigger difficult problem always.Traditional antifouling protective system utilizes toxicants such as Red copper oxide or tin class to suppress adhering to of marine life and grows, but these toxicants have caused severe contamination to seawater.Therefore, seek the direction that novel antifouling anticorrosive coating nontoxic, high Corrosion Protection has become people's research.
Polypyrrole (Ppy) is a kind of nontoxic conductive polymers that has excellent conducting performance, chemical stability, light stability and prepare easily.Polynite (MMT) is made up of the thick silicate lamella of about 1nm, and lamella is made up of silicon-oxy tetrahedron and alumina octahedral, and interlayer is kept balance by the absorption positively charged ion.Polynite (MMT) has characteristics such as nanometer size effect, surface interface effect, quantum size effect, macro quanta tunnel effect.The compound conductive polymers based nano composite material that obtains of inorganic laminated thing or ultrapureization, superfine inorganic particulate and conductive polymers.Polynite is a kind of inertia main body that does not have oxidizing property, thereby monomer can be inserted between the stratiform lamella or space of polynite, it is peeled off become the nanometer lamella, thereby be evenly dispersed in the polymeric matrix, and the adding doping agent can improve the electron distributions situation of polymer chain, thereby improved the conductivity of polymkeric substance, realized the highly corrosion resistant performance of matrix material.
At present, existing many investigators study nano imvite and polypyrrole mixture and the Corrosion Protection that conducts electricity thereof.Zhao Jinling, and Wang Lixin etc. [Zhao Jinling etc. the preparation of polypyrrole/montmorillonite composite material and performance [J]. polymer material science and engineering, 2003,19 (4)] be medium with water, FeCl
3Be oxygenant, prepared polypyrrole/montmorillonite composite material with chemical oxidization method.Studied the influence to polyreaction of temperature of reaction, reaction times, polynite and factors such as oxygenant consumption, dopant species and consumption, the specific conductivity of the matrix material of preparation has reached 50.0S/cm in the time of 0 ℃, and in the 50d, low temperature product specific conductivity is declined by less than 10%.Su Haixia, Ceng Xingrong [Chinese patent, CN1597769A, polypyrrole/organic montmorillonite nano composite material and its production and application] has reported with iron trichloride (FeCl
3) be oxygenant, paratoluenesulfonic acid sodium salt (TSANa) is a doping agent, make to enter oxidative polymerization takes place, join in the epoxy curing agent, prepared and have the electrostatic aqueous epoxy coating of good resistance through the pyrroles (Py) of organic intercalation agent montmorillonite modified (OMMT) interlayer.Li Lan, [Chinese patent such as Ji Xu, CN1375534A, nano montmorillonoid modified paint and its production and use] introduced a kind of nano montmorillonoid modified paint as the preparation method of automobile finish, with the polynite of nanometer organic active as filler, joining hydroxyl alkyd resins is in the main film forming substance, adds modified resin, pigment and other auxiliary agents such as aminoresin again, forms through mixing, grind, be in harmonious proportion, filtering.Because features such as the surfactivity of nanometer organic active polynite particle, interfacial effect make interparticle autohemagglutination effect reduce, and have improved the fullness ratio and the clarity of filming, and with the tack of ground.Li Chunzhong, [Chinese patent such as Gu Zheming, CN101544823A, a kind of matrix material and preparation method thereof with high conductivity intercalation structure] introduced a kind of preparation method of polypyrrole/oxidized graphite composite material of intercalation configuration, earlier graphite oxide is dispersed in the aqueous hydrochloric acid of PH=1～3, add the tensio-active agent cetyl trimethylammonium bromide again, ultrasonication 30～60min under the room temperature, obtain colloidal dispersion, pyrrole monomer is added wherein, through magnetic agitation, add ammonium persulphate and carry out letex polymerization 3～24h, after suction filtration at 0～5 ℃, washing, obtain intercalation configuration polypyrrole/graphite oxide composite that electric conductivity only is 4～5S/cm after the drying.[Chinese patent such as Pan Caiyuan, CN100999558A, the surface controllable polymerization prepares the method for nano composite polymer-montmorillonoid material] reported a kind of surperficial controllable polymerization that utilizes, vinylbenzene, esters of acrylic acid or basic esters of acrylic acid or acrylic acid amides class or monomers such as methacrylic acid amides, vinyl pyridine are contained at initiator, interlayer under the polynite condition of chain-transfer agent reversible fracture chain transfer polymerization reaction takes place, prepare the polymer-montmorillonoid matrix material.The tensile strength of this kind material, thermostability, solvent resistance and flame retardant resistance increase.
In existing report, do not see that the nano imvite and the polypyrrole mixture that utilize intercalation configuration prepare high Corrosion Protection water-borne coatings.
Summary of the invention
The object of the present invention is to provide a kind of nano imvite and polypyrrole mixture watery anti-corrosion paint and preparation method thereof.
The raw material of described nano imvite and polypyrrole mixture watery anti-corrosion paint is formed and by the content of mass ratio is:
Polynite 1～50, solvent 20～300, protonic acid 0.8～55, organic activator 0.07～18.5, Iron(III) chloride hexahydrate (FeCl
36H
2O) or ferric sulfate (Fe
2(SO
4)
3) 8.5～50.6, the pyrroles 0.8～56, tensio-active agent 4.5～50, matrix resin 10～55, modified resin 0～10, neutralizing agent 0.34～5.6, pigment 0.6～10, deionized water 20～100, defoamer 0.05～1.2, anti-settling agent 0.22～1.34, dispersion agent 0.13～115, flow agent 0.02～1.08, film coalescence aid 0.05～1.04.
Described solvent can be selected from least a in distilled water, alcohols, acetone, chloroform or the aliphatics acids etc.
Described protonic acid can be selected from least a in hydrochloric acid, phosphoric acid, sulfuric acid, acetic acid, sulfonic acid, the phthalic acid etc.
Described organic activator (this reagent can pass through the chemical constitution on the surface of change inorganic mineral, makes it to be easy to disperse absorption) can be selected from diamine, tertiary amine or cerous sulfate (Ce (SO
4)
2) at least a in waiting.
Described tensio-active agent can be selected from least a in dimer phosphoric acid salt of triphen ethyl phenol polyoxyethylene ether phosphate, bis-alkoxy Diphosphonate, Phosphate of Polyoxyethylene Isooctyl Ether salt, butyl-a-D-glycopyranoside etc.
Described modified resin can be selected from least a in resol, urea-formaldehyde resin, melamine resin, acrylic resin, the resol etc.;
Described neutralizing agent can be selected from least a in monoamine, diamine, the ternary amine etc.
Described pigment can be selected from least a in titanium dioxide, carbon black, barium sulfate, talcum powder, the lime carbonate etc.
Described defoamer can be selected from silicone based defoamer (model: BYK302, BYK065, BYK20) that low mass molecule alcohol class, phosphoric acid ester, silicone emulsion class, German Bi Ke company produce, inorganic silicon defoamer (model: BYK011, BYK053) that German Bi Ke company produces, antifoaming agent of non-silicone that EFKA company produces (model: at least a Efka2018) or in the defoamer (model: SPA102, SPA202) produced with power development in science and technology company limited of Shanghai etc.
Described anti-settling agent can be selected from least a in titanate coupling agent, aerosil, wilkinite, the Walocel MT 20.000PV etc.
Described dispersion agent can be selected from least a in sodium oleate, sodium polyphosphate, sodium alkyl sulfate, polyoxyethylene carboxylate, alkylphenol polyvinyl ether, octadecyl dimethyl betaine, the soybean lecithin sodium polymethacrylate etc.;
Described flow agent can be selected from least a in the organosilicon flow agent (model: BYK306, BYK310, BYK356, BYK390) that ethylene glycol monobutyl ether, water-soluble ether-ether, polydimethylsiloxane, German Bi Ke company produce etc.
Described film coalescence aid can be selected from least a in butyl Bian alcohol acetic ester, butyl glycol ether carboxylic ester, ethylene glycol phenyl ether, dibasic acid dimethyl ester, propylene glycol propyl ether, the diprotic acid diethyl ester class etc.
Described matrix resin can be selected from least a in aqueous epoxy resins, urethane resin, aminoresin, acrylic resin, Synolac, the vibrin etc.
The preparation method of described nano imvite and polypyrrole mixture watery anti-corrosion paint may further comprise the steps:
(1) preparation of nano imvite and polypyrrole mixture
1) pre-treatment of polynite
Polynite is added in distilled water or the organic solvent disperses, under 40～80 ℃, stir through the speed of stirrer with 600～1000r/min, form suspension system, leave standstill 24h, remove the impurity of no swelling in the polynite, protonic acid is joined again and carry out the proton activation effect in the suspension, it is standby to form suspension; The dispersion soln that again organic activator is dissolved in distilled water or the organic solvent slowly is added drop-wise in the standby suspension, stir 0.5～4h, centrifugation 1～3h again, obtain the nanometer organic active montmorillonite suspension liquid of intercalation configuration, after leaving standstill, drying is ground the back and is crossed 100 mesh sieves, obtains the nanometer organic active polynite powder of size of particles at the intercalation configuration of 10～100nm;
2) nano imvite and polypyrrole mixture is synthetic
Under condition of ice bath, with FeCl
36H
2O or Fe
2(SO
4)
3Be dissolved in the redistilled water, add tensio-active agent and form suspension, add nanometer organic active polynite powder again, stir, inject pyrrole monomer, the rapid blackening of system, under nitrogen protection, reaction 12～24h, reaction finishes the back and carries out ultra-sonic dispersion earlier in water, carries out centrifugation again, the precipitate with deionized water repetitive scrubbing of gained, be neutral until filtrate, the gained precipitation is dry, obtain nano imvite and polypyrrole composite powder through grinding;
(2) preparation of nano imvite and polypyrrole mixture watery anti-corrosion paint
1) get above-mentionedly based on nano imvite and polypyrrole composite powder, mix with matrix resin, modified resin, neutralizing agent, deionized water, homodisperse 1～4h on dispersion machine obtains green dispersion system;
2) get pigment, defoamer, dispersion agent, flow agent, anti-settling agent, film coalescence aid and add green dispersion system, dispersed with stirring 1～4h filters and promptly obtains nano imvite and polypyrrole mixture watery anti-corrosion paint.
The present invention has following characteristics:
1) utilizes highly active phosphoric acid salt Gemini surface active agent (containing two hydrophilic heads of two hydrophobic chains and the gentle or basic tensio-active agent that is rigidly connected in the molecule) activation polynite, by synthetic significant nano imvite of intercalation effect of chemical oxidization method and polypyrrole mixture, prepare watery anti-corrosion paint with this as conductive filler material again.Compare with tensio-active agents such as the benzene sulfonic acid sodium salt of routine or hexadecyl bromination ammonium salts, the organic phosphoric acid salt cation has greatly changed the polarity of montmorillonite layer, reduced the surface energy of montmorillonite layer, increased by two alternate affinities, its intercalation effect has improved several times.Preparation method of the present invention is simple, compares with conductive anti-corrosion coatings such as single polypyrrole, polyanilines, and electric conductivity is significantly improved, and Corrosion Protection obviously strengthens.In addition, advantage of the present invention is that also this kind coating also has antifouling, antistatic effect.
2) utilize conductive polymers at nano imvite interlayer initiated polymerization, nano imvite of preparing and polypyrrole mixture watery anti-corrosion paint surface resistivity are low, have the characteristic of high conductivity, and Corrosion Protection improves greatly.
3) this coating has good heat resistance, chemical mediator performances such as acid-and base-resisting.
4) this preparation method for coating is simple, and is with low cost, and unharmful substance meets relevant national standard.
Description of drawings
Fig. 1 is the nano imvite of the embodiment of the invention 1 preparation and the TEM figure of polypyrrole mixture watery anti-corrosion paint.In Fig. 1, scale is 20nm.
Fig. 2 is the nano imvite of the embodiment of the invention 2 preparations and the TEM figure of polypyrrole mixture watery anti-corrosion paint.In Fig. 2, scale is 20nm.
Fig. 3 is the nano imvite of the embodiment of the invention 3 preparations and the TEM figure of polypyrrole mixture watery anti-corrosion paint.In Fig. 3, scale is 50nm.
Fig. 4 is the nano imvite of the embodiment of the invention 4 preparations and the TEM figure of polypyrrole mixture watery anti-corrosion paint.In Fig. 4, scale is 50nm.
Fig. 5 is the nano imvite of the embodiment of the invention 5 preparations and the TEM figure of polypyrrole mixture watery anti-corrosion paint.In Fig. 5, scale is 20nm.
Embodiment
Embodiment 1
Step 1 is added to the 1g polynite in the 20mL ethanol, stirs through the speed of stirrer with 800r/min under 60 ℃, forms suspension system, leaves standstill 24h, removes the impurity of no swelling in the polynite.0.8mL sulfuric acid is joined in the suspension, it is standby to form suspension again; The 2mL quadrol being dissolved in the 15mL ethanolic soln slowly is added drop-wise in the standby suspension again, stir 1h while dripping, centrifugation obtains the nanometer organic active montmorillonite suspension liquid of intercalation configuration again, leave standstill a night, at 60 ℃ of following vacuum-drying 12h, grind the back and cross 100 mesh sieves, obtain the nanometer organic active polynite powder of size of particles at the intercalation configuration of 10～100nm.
Step 2, under condition of ice bath, with 0.8gFeCl
36H
2O is dissolved in the 20mL redistilled water, adds 4.5g triphen ethyl phenol polyoxyethylene ether phosphate and forms suspension, adds 1g nanometer organic active polynite powder again; stir, inject 0.80mL pyrrole monomer, the rapid blackening of system with syringe; under nitrogen protection, reaction 20h.Reaction finishes the back and carries out ultra-sonic dispersion earlier in water, carries out centrifugation 1h again, and the precipitate with deionized water repetitive scrubbing of gained is neutral until filtrate.Gained is deposited in 60 ℃ of following vacuum-drying 24h, obtains nano imvite and polypyrrole composite powder through grinding.
Step 3, get above-mentioned nano imvite of 1.0g and polypyrrole composite powder, mix with 20g aqueous alkide resin, 1g resol, 0.34g ammoniacal liquor, 20mL deionized water, homodisperse 2h on high speed dispersor obtains a green dispersion system.
Step 4, get 0.6g talcum powder, 0.05g SPA102,0.03g sodium alkyl sulfate, 0.02g ethylene glycol monobutyl ether, 0.22g titanate coupling agent, 0.05g propylene glycol propyl ether adds above-mentioned system, even dispersed with stirring 2h, filtration can obtain nano imvite and polypyrrole mixture watery anti-corrosion paint.
Embodiment 2
Step 1, the 12g polynite is added in the 40mL ethanol, under 60 ℃, stirs, form suspension system, leave standstill 24h, remove the impurity of no swelling in the polynite through the speed of stirrer with 800r/min.10mL sulfuric acid is joined in the suspension, it is standby to form suspension again; Again with 15mL Ce (SO
4)
2Being dissolved in 200mLDMF solution slowly is added drop-wise in the standby suspension, stir 3h while dripping, centrifugation obtains the nanometer organic active montmorillonite suspension liquid of intercalation configuration again, leave standstill a night, at 60 ℃ of following vacuum-drying 20h, grind the back and cross 100 mesh sieves, obtain the nanometer organic active polynite powder of size of particles at the intercalation configuration of 10～100nm.
Step 2, under condition of ice bath, with 15gFeCl
36H
2O is dissolved in the 50mL redistilled water, adds 11.5g bis-alkoxy Diphosphonate and forms suspension, adds 7.5g nanometer organic active polynite powder again; stir, inject 10mL pyrrole monomer, the rapid blackening of system with syringe; under nitrogen protection, reaction 20h.Reaction finishes the back and carries out ultra-sonic dispersion earlier in water, carries out centrifugation again, and the precipitate with deionized water repetitive scrubbing of gained is neutral until filtrate.Gained is deposited in 60 ℃ of following vacuum-drying 20h, obtains nano imvite and polypyrrole composite powder through grinding.
Step 3, get above-mentioned nano imvite of 10g and polypyrrole composite powder, mix with 25g aqueous epoxy resins, 4.5g urea-formaldehyde resin, 3.5g (concentration is 28%) oxyammonia, 50mL deionized water, homodisperse 4h on high speed dispersor obtains a green dispersion system.
Step 4, get 3g lime carbonate, 0.2g BYK11,0.35g sodium polyphosphate, 0.32g polydimethylsiloxane, 0.53g aerosil, 0.40g ethylene glycol phenyl ether adds above-mentioned system, even dispersed with stirring 2h, filtration can obtain nano imvite and polypyrrole mixture watery anti-corrosion paint.
Embodiment 3
Step 1, the 25g polynite is added in the 60mL ethanol, under 60 ℃, stirs, form suspension system, leave standstill 24h, remove the impurity of no swelling in the polynite through the speed of stirrer with 800r/min.25mL sulfuric acid is joined in the suspension, it is standby to form suspension again; The 30mL triethylamine being dissolved in the 65mL ethanolic soln slowly is added drop-wise in the standby suspension again, stir 3h while dripping, centrifugation obtains the nanometer organic active montmorillonite suspension liquid of intercalation configuration again, leave standstill a night, at 60 ℃ of following vacuum-drying 24h, grind the back and cross 100 mesh sieves, obtain the nanometer organic active polynite powder of size of particles at the intercalation configuration of 10～100nm.
Step 2, under condition of ice bath, with 28gFe
2(SO
4)
3Be dissolved in the 60mL redistilled water, add 10g Phosphate of Polyoxyethylene Isooctyl Ether salt formation suspension, add 1g nanometer organic active polynite powder again; stir, inject 2mL pyrrole monomer, the rapid blackening of system with syringe; under nitrogen protection, reaction 20h.Reaction finishes the back and carries out ultra-sonic dispersion earlier in water, carries out centrifugation 2h again, and the precipitate with deionized water repetitive scrubbing of gained is neutral until filtrate.Gained is deposited in 60 ℃ of following vacuum-drying 24h, obtains nano imvite and polypyrrole composite powder through grinding.
Step 3, get above-mentioned nano imvite of 22g and polypyrrole composite powder, mix with 30g water-based alkyd resin, 4.5g melamine resin, 1.2g dimethylethanolamine, 60mL deionized water, homodisperse 3h on high speed dispersor obtains a green dispersion system.
Step 4, get 4.5g titanium dioxide, 0.42gEfka2018,0.48g octadecyl dimethyl betaine, 0.5gBYK365,0.7g titanate coupling agent, 0.43g the butyl glycol ether carboxylic ester adds above-mentioned system, even dispersed with stirring 3h, filtration can obtain nano imvite and polypyrrole mixture watery anti-corrosion paint.
Embodiment 4
Step 1, the 35g polynite is added in the 80mL ethanol, under 60 ℃, stirs, form suspension system, leave standstill 24h, remove the impurity of no swelling in the polynite through the speed of stirrer with 800r/min.42mL sulfuric acid is joined in the suspension, it is standby to form suspension again; The 40mL quadrol being dissolved in slowly is added drop-wise in the standby suspension again in the 70mL redistilled water, stir 3h while dripping, centrifugation obtains the nanometer organic active montmorillonite suspension liquid of intercalation configuration again, leave standstill a night, at 60 ℃ of following vacuum-drying 32h, grind the back and cross 100 mesh sieves, obtain the nanometer organic active polynite powder of size of particles at the intercalation configuration of 10～100nm.
Step 2, under condition of ice bath, with 36gFe
2(SO
4)
39H
2O is dissolved in the 200mL redistilled water, adds 19.2g Phosphate of Polyoxyethylene Isooctyl Ether salt formation suspension, adds 1g nanometer organic active polynite powder again; stir, inject 2mL pyrrole monomer, the rapid blackening of system with syringe; under nitrogen protection, reaction 20h.Reaction finishes the back and carries out ultra-sonic dispersion earlier in water, carries out centrifugation again, and the precipitate with deionized water repetitive scrubbing of gained is neutral until filtrate.Gained is deposited in 60 ℃ of following vacuum-drying 24h, obtains nano imvite and polypyrrole composite powder through grinding.
Step 3, get above-mentioned nano imvite of 25g and polypyrrole composite powder, mix with 40g waterborne polyurethane resin, 5g acrylic resin, 3.2g Triethylenetetramine (TETA), 70mL deionized water, homodisperse 3h on high speed dispersor obtains a green dispersion system.
Step 4, get 7.5g lime carbonate, 0.88g BYK065,0.65g soybean lecithin sodium polymethacrylate, 0.72g ethylene glycol monobutyl ether, 0.69g Walocel MT 20.000PV, 0.46g propylene glycol propyl ether adds above-mentioned system, even dispersed with stirring 3.5h, filtration can obtain nano imvite and polypyrrole mixture watery anti-corrosion paint.
Embodiment 5
The pre-treatment of step 1, polynite
The 55g polynite is added in the 100mL ethanol, under 60 ℃, stirs, form suspension system, leave standstill 24h, remove the impurity of no swelling in the polynite through the speed of stirrer with 700r/min.55mL sulfuric acid is joined in the suspension, it is standby to form suspension again; The 30mL triethylamine being dissolved in the 100mL ethanolic soln slowly is added drop-wise in the standby suspension again, stir 3h while dripping, centrifugation 3h again, obtain the nanometer organic active montmorillonite suspension liquid of intercalation configuration, leave standstill a night, at 60 ℃ of following vacuum-drying 24h, grind the back and cross 100 mesh sieves, obtain the nanometer organic active polynite powder of size of particles at the intercalation configuration of 10～100nm.
Step 2, under condition of ice bath, with 50.6gFeCl
36H
2O is dissolved in the 500mL redistilled water, and the dimer phosphoric acid salt that adds 50g butyl-a-D-glycopyranoside forms suspension, adds 50g nanometer organic active polynite powder again; stir, inject 6mL pyrrole monomer, the rapid blackening of system with syringe; under nitrogen protection, reaction 20h.Reaction finishes the back and carries out ultra-sonic dispersion earlier in water, carries out centrifugation 3h again, and the precipitate with deionized water repetitive scrubbing of gained is neutral until filtrate.Gained is deposited in 60 ℃ of following vacuum-drying 24h, obtains nano imvite and polypyrrole composite powder through grinding.
Step 3, get above-mentioned nano imvite of 50g and polypyrrole composite powder, mix with 55g water-borne acrylic resin, 10g resol, 5.6g ammoniacal liquor, 100mL deionized water, homodisperse 3h on high speed dispersor obtains a green dispersion system.
Step 4, get 1g talcum powder, 1.2g SPA102,1.15g sodium oleate, 1.08g polydimethylsiloxane, 1.34g titanate coupling agent, 1.04g butyl Bian alcohol acetic ester adds above-mentioned system, even dispersed with stirring 4h, filtration can obtain nano imvite and polypyrrole mixture watery anti-corrosion paint.
The product of above-mentioned 5 embodiment is analyzed through the JEM-2100 high-resolution-ration transmission electric-lens, and the result can see the polypyrrole that utilizes different components content in the polymerization of nano imvite interlayer shown in Fig. 1～5, and its interlamellar spacing obviously increases.
Through dependence test, gained nano imvite and polypyrrole mixture watery anti-corrosion paint embodiment properties of sample test result see Table 1 with the above-mentioned embodiment sample that obtains.
Table 1
Claims (10)
1. nano imvite and polypyrrole mixture watery anti-corrosion paint, it is characterized in that its raw material is formed and be: polynite 1～50 by the content of mass ratio, solvent 20～300, protonic acid 0.8～55, organic activator 0.07～18.5, Iron(III) chloride hexahydrate or ferric sulfate 8.5～50.6, the pyrroles 0.8～56, tensio-active agent 4.5～50, matrix resin 10～55, modified resin 0～10, neutralizing agent 0.34～5.6, pigment 0.6～10, deionized water 20～100, defoamer 0.05～1.2, anti-settling agent 0.22～1.34, dispersion agent 0.13～115, flow agent 0.02～1.08, film coalescence aid 0.05～1.04.
2. nano imvite as claimed in claim 1 and polypyrrole mixture watery anti-corrosion paint is characterized in that described solvent is selected from least a in distilled water, alcohols, acetone, chloroform or the aliphatics acids; Described protonic acid is selected from least a in hydrochloric acid, phosphoric acid, sulfuric acid, acetic acid, sulfonic acid, the phthalic acid.
3. nano imvite as claimed in claim 1 and polypyrrole mixture watery anti-corrosion paint is characterized in that described organic activator is selected from least a in diamine, tertiary amine or the cerous sulfate.
4. nano imvite as claimed in claim 1 and polypyrrole mixture watery anti-corrosion paint is characterized in that described tensio-active agent is selected from least a in the dimer phosphoric acid salt of triphen ethyl phenol polyoxyethylene ether phosphate, bis-alkoxy Diphosphonate, Phosphate of Polyoxyethylene Isooctyl Ether salt, butyl-a-D-glycopyranoside.
5. nano imvite as claimed in claim 1 and polypyrrole mixture watery anti-corrosion paint is characterized in that described modified resin is selected from least a in resol, urea-formaldehyde resin, melamine resin, acrylic resin, the resol.
6. nano imvite as claimed in claim 1 and polypyrrole mixture watery anti-corrosion paint is characterized in that described neutralizing agent is selected from least a in monoamine, diamine, the ternary amine; Described nano imvite and polypyrrole mixture watery anti-corrosion paint is characterized in that described pigment is selected from least a in titanium dioxide, carbon black, barium sulfate, talcum powder, the lime carbonate.
7. nano imvite as claimed in claim 1 and polypyrrole mixture watery anti-corrosion paint is characterized in that described defoamer is selected from least a in low mass molecule alcohol class, phosphoric acid ester, silicone emulsion class, silicone based defoamer, inorganic silicon defoamer, the antifoaming agent of non-silicone; Described anti-settling agent is selected from least a in titanate coupling agent, aerosil, wilkinite, the Walocel MT 20.000PV; Described dispersion agent is selected from least a in sodium oleate, sodium polyphosphate, sodium alkyl sulfate, polyoxyethylene carboxylate, alkylphenol polyvinyl ether, octadecyl dimethyl betaine, the soybean lecithin sodium polymethacrylate etc.
8. nano imvite as claimed in claim 1 and polypyrrole mixture watery anti-corrosion paint is characterized in that described flow agent is selected from least a in ethylene glycol monobutyl ether, water-soluble ether-ether, polydimethylsiloxane, the organosilicon flow agent; Described film coalescence aid is selected from least a in butyl Bian alcohol acetic ester, butyl glycol ether carboxylic ester, ethylene glycol phenyl ether, dibasic acid dimethyl ester, propylene glycol propyl ether, the diprotic acid diethyl ester class.
9. nano imvite as claimed in claim 1 and polypyrrole mixture watery anti-corrosion paint is characterized in that described matrix resin is selected from least a in aqueous epoxy resins, urethane resin, aminoresin, acrylic resin, Synolac, the vibrin.
10. the preparation method of nano imvite as claimed in claim 1 and polypyrrole mixture watery anti-corrosion paint is characterized in that may further comprise the steps:
(1) preparation of nano imvite and polypyrrole mixture
1) pre-treatment of polynite
Polynite is added in distilled water or the organic solvent disperses, under 40～80 ℃, stir through the speed of stirrer with 600～1000r/min, form suspension system, leave standstill 24h, remove the impurity of no swelling in the polynite, protonic acid is joined again and carry out the proton activation effect in the suspension, it is standby to form suspension; The dispersion soln that again organic activator is dissolved in distilled water or the organic solvent slowly is added drop-wise in the standby suspension, stir 0.5～4h, centrifugation 1～3h again, obtain the nanometer organic active montmorillonite suspension liquid of intercalation configuration, after leaving standstill, drying is ground the back and is crossed 100 mesh sieves, obtains the nanometer organic active polynite powder of size of particles at the intercalation configuration of 10～100nm;
2) nano imvite and polypyrrole mixture is synthetic
Under condition of ice bath, with FeCl
36H
2O or Fe
2(SO
4)
3Be dissolved in the redistilled water, add tensio-active agent and form suspension, add nanometer organic active polynite powder again, stir, inject pyrrole monomer, the rapid blackening of system, under nitrogen protection, reaction 12～24h, reaction finishes the back and carries out ultra-sonic dispersion earlier in water, carries out centrifugation again, the precipitate with deionized water repetitive scrubbing of gained, be neutral until filtrate, the gained precipitation is dry, obtain nano imvite and polypyrrole composite powder through grinding;
(2) preparation of watery anti-corrosion paint
1) get above-mentionedly based on nano imvite and polypyrrole composite powder, mix with matrix resin, modified resin, neutralizing agent, deionized water, homodisperse 1～4h on dispersion machine obtains green dispersion system;
2) get pigment, defoamer, dispersion agent, flow agent, anti-settling agent, film coalescence aid and add green dispersion system, dispersed with stirring 1～4h filters and promptly obtains nano imvite and polypyrrole mixture watery anti-corrosion paint.
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